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目的建立毛细管气相色谱法测定帕司烟肼中的残留溶剂乙醇和异丙醇的含量。方法采用气相色谱法测定,色谱柱为Agilent DB-624毛细管色谱柱(30.0 m×0.32 mm×1.4μm),载气为氮气,FID检测器,采用顶空进样,程序升温,按外标法计算残留溶剂含量。结果乙醇和异丙醇分别在50.66~151.97μg/m L和49.23~147.69μg/m L范围内呈良好的线性关系(r=0.999 9,n=5);乙醇、异丙醇加样回收率分别达到99.7%、99.5%;仪器精密度高,乙醇、异丙醇峰RSD均为1.0%(n=6);稳定性好,24 h间隔进样乙醇、异丙醇峰面积RSD分别为0.86%、0.14%。结论本方法简单、灵敏、可靠,适用于帕司烟肼中残留溶剂的分析检测。
Objective To establish a capillary gas chromatographic method for the determination of residual solvents ethanol and isopropanol in attapulginazide. Methods The gas chromatography was used. The chromatographic column was Agilent DB-624 capillary column (30.0 m × 0.32 mm × 1.4 μm). The carrier gas was nitrogen and FID detector. The headspace sampling was used and the temperature was programmed. Calculate residual solvent content. Results There was a good linear relationship between ethanol and isopropanol in the range of 50.66 ~ 151.97μg / ml and 49.23 ~ 147.69μg / ml respectively (r = 0.999 9, n = 5) Respectively. The RSD of ethanol and isopropanol were all 1.0% (n = 6). The stability was good. The peak area RSD of ethanol and isopropanol at 24 h intervals were 0.86 %, 0.14%. Conclusion The method is simple, sensitive and reliable, suitable for the analysis and determination of residual solvents in paroxysm.